Citation: | WU Yanyan, LIU Fajia, LI Laihao, YANG Xianqing, DENG Jianchao, CHEN Shengjun, MA Haixia. Determination and optimization of N-nitrosamines in salted fish by gas chromatography-mass spectrometry[J]. South China Fisheries Science, 2012, 8(4): 16-22. DOI: 10.3969/j.issn.2095-0780.2012.04.003 |
We determined N-nitrosamines in salted fish by gas chromatography-mass spectrometry (GC-MS), optimized the sample preparation conditions, compared the response intensity of N-nitrosamines by SPME and dichloromethane ultrasonic extraction as well as explored the impact of organic solvent, extraction time and times on the determination. By ion selective electrode method, we determined the contents of N-dimethylnitrosamine, N-diethylnitrosamine, N-nitroso-pyrrolidine and N-nitrosamines. Results show that the linear correlation coefficient is 0.999 2, 0.999 1, 0.999 1 and 0.999 2, respectively, with a linear range of 0~10 μg·mL-1. The method has good reproducibility (RSD≤2.1%, blank spiked recovery is 70%~80%) and high sensitivity (detection limit is 0.038 6 μg·kg-1, 0.022 7 μg·kg-1, 0.031 6 μg·kg-1 and 0.047 8 μg·kg-1, respectively).
[1] |
何计国, 甄润英. 食品卫生学[M]. 北京: 中国农业大学出版社, 2003: 89-100.
HE Jiguo, ZHEN Runying. Food hygiene[M]. Beijing: China Agricultural University Press, 2003: 89-100. (in Chinese)
|
[2] |
胡丽芳, 尹德凤, 周瑶敏, 等. 气质联用法测定咸鱼中N-二甲基亚硝胺含量[J]. 江西农业学报, 2009, 21(9): 135-136. doi: 10.3969/j.issn.1001-8581.2009.09.044
HU Lifang, YIN Defeng, ZHOU Yaomin, et al. Determination of N-dimethylnitrosamine in salt fish by gas chromatography-mass spectrometry[J]. Acta Agriculturae Jiangxi, 2009, 21(9): 135-136. (in Chinese) doi: 10.3969/j.issn.1001-8581.2009.09.044
|
[3] |
丁红梅, 陈彬, 杨兴龙, 等. 气质联用法测定生食水产品中挥发性N-亚硝胺[J]. 食品与机械, 2010, 26(6): 54-69. doi: 10.3969/j.issn.1003-5788.2010.06.016
DING Hongmei, CHEN Bin, YANG Xinglong, et al. Determination of volatile raw aquatic products of N-nitrosaminesby gas chromatography-mass pectrometry[J]. Food Machinery, 2010, 26(6): 54-69. (in Chinese) doi: 10.3969/j.issn.1003-5788.2010.06.016
|
[4] |
马俪珍, 南庆贤, 方长法. N-亚硝胺类化合物与食品安全性[J]. 农产品加工学刊, 2005(12): 8-12. doi: 10.3969/j.issn.1671-9646-B.2005.12.002
MA Lizhen, NAN Qingxian, FANG Changfa. N-nitrosmine compounds and food safety[J]. Farm Prod Process, 2005(12): 8-12. (in Chinese) doi: 10.3969/j.issn.1671-9646-B.2005.12.002
|
[5] |
MITACEK E J, BRUNNEMANN K D, SUTTAJIT M, et al. Exposureto N-nitroso compounds in a population of high liver cancer regions in Thailand: volatilenitrosa-mine (VNA) levels in Thaifood[J]. Food Chem Toxicol, 1999, 37(4): 297-305. doi: 10.1016/S0278-6915(99)00017-4
|
[6] |
蔡一新, 林升清, 林生金. 福建省部分食品中N-亚硝胺含量调查结果分析[J]. 中国卫生检验杂志, 1997, 7(6): 356-358. https://kns.cnki.net/kcms2/article/abstract?v=MdENDFpkZq4mw_wziPZc4tmbuCvY97oWlxoY9Y0_nKBSq8g3DSW6GKZ--hrKnJbklzW1OeaBBXuGfnxiBBOvaUtWrY_HFcVQ62E1ZOLuSnJgBcd1mKdxzM5UGk93fZbpPKufFwp4YZv2KqDIAdmTXwvC4J4q9Er7YUCSKQw1du6c8gkZlbNbg1gCs4l42Uie&uniplatform=NZKPT&language=CHS
CAI Yixin, LIN Shengqing, LIN Shengjin. N-nitrosamine content analysis of the survey in part of the food from Fujian province[J]. Chin J Health Lab Technol, 1997, 7(6): 356-358. (in Chinese) https://kns.cnki.net/kcms2/article/abstract?v=MdENDFpkZq4mw_wziPZc4tmbuCvY97oWlxoY9Y0_nKBSq8g3DSW6GKZ--hrKnJbklzW1OeaBBXuGfnxiBBOvaUtWrY_HFcVQ62E1ZOLuSnJgBcd1mKdxzM5UGk93fZbpPKufFwp4YZv2KqDIAdmTXwvC4J4q9Er7YUCSKQw1du6c8gkZlbNbg1gCs4l42Uie&uniplatform=NZKPT&language=CHS
|
[7] |
樊丽琴. 咸鱼腌制过程中N-亚硝胺及其前体物质的变化规律研究[D]. 湛江: 广东海洋大学, 2009: 16-17. 10.7666/d.y1552051
FAN Liqin. Study on the changing regularity of N-nitrosamine and its precursor substance in pickling salted fish[D]. Zhanjiang: Guangdong Ocean University, 2009: 16-17. (in Chinese) 10.7666/d.y1552051
|
[8] |
刘法佳, 吴燕燕, 李来好, 等. 降低腌制食品中亚硝酸盐含量的研究进展[J]. 广东农业科学, 2011, 38(1): 165-167. doi: 10.3969/j.issn.1004-874X.2011.01.061
LIU Fajia, WU Yanyan, LI Laihao, et al. Development of reducing of nitrite in salted food[J]. Guangdong Agric Sci, 2011, 38 (1): 165-167. (in Chinese) doi: 10.3969/j.issn.1004-874X.2011.01.061
|
[9] |
吴燕燕, 刘法佳, 李来好, 等. 改良离子色谱法测定咸鱼中亚硝酸盐的研究[J]. 南方水产科学, 2011, 7(6): 1-6. doi: 10.3969/j.issn.2095-0780.2011.06.001
WU Yanyan, LIU Fajia, LI Laihao, et al. Determination of nitrite in salted fishes by the improved ion chromatography[J]. South China Fish Sci, 2011, 7(6): 1-6. (in Chinese) doi: 10.3969/j.issn.2095-0780.2011.06.001
|
[10] |
孙效晖, 韩一鸣, 林弟雄, 等. GB 10138-2005盐渍鱼卫生标准[S]. 北京: 中国标准出版社, 2005.
SUN Xiaohui, HAN Yiming, LIN Dixiong, et al. GB 10138-2005. Hygienic standard for salted fish[S]. Beijing: Standards Press of China, 2005. (in Chinese)
|
[11] |
魏法山, 徐幸莲, 周光宏. 挥发性N-亚硝基化合物的分析方法[J]. 食品科学, 2008, 29(7): 479-483. doi: 10.3321/j.issn:1002-6630.2008.07.109
WEI Fashan, XU Xinglian, ZHOU Guanghong. Determination method of volatile N-nioso compounds[J]. Food Sci, 2008, 29(7): 479-483. (in Chinese) doi: 10.3321/j.issn:1002-6630.2008.07.109
|
[12] |
王瑞, 马俪珍, 方长发. 毛细管气相色谱法对冷却猪肉中挥发性N-亚硝胺类化合物含量的测定分析[J]. 天津农学院学报, 2006, 13(1): 10-13. doi: 10.3969/j.issn.1008-5394.2006.01.003
WANG Rui, MA Lizhen, FANG Changfa. Application of gas chromatography by capillary tube to determine volatilizable N-nitrosamine compound in cooled pork[J]. J Tianjin Agric Univ, 2006, 13(1): 10-13. (in Chinese) doi: 10.3969/j.issn.1008-5394.2006.01.003
|
[13] |
张秋菊, 郭祖鹏, 李明珠, 等. 顶空固相微萃取-气相色谱-质谱法测定7种亚硝胺类化合物[J]. 中国卫生检验杂志, 2009, 19(6): 1234-1236. https://kns.cnki.net/kcms2/article/abstract?v=MdENDFpkZq4nArXXU3X4WZc8ylJDUb7tavi5rIpoDQQadAKBvKGcvCNgCMlT5mMG03FD4NyoQyFfCZ9w76HiyMZJg6cwsS5-VtJg1Rs1xG80md1B8DrUGrSp8YeIBpxbrmK_8wpQPWjkMQdJQPpUX4FAOyq5Nt1Y1MbrEjd8j68CG15mtG8yWmnMrz3shNSf&uniplatform=NZKPT&language=CHS
ZHANG Qiuju, GUO Zupeng, LI Ming zhu, et al. Determination of seven N-nitrosamine compounds by HS-SPME-GC-MS[J]. Chin J Health Lab Technol, 2009, 19(6): 1234-1236. (in Chinese) https://kns.cnki.net/kcms2/article/abstract?v=MdENDFpkZq4nArXXU3X4WZc8ylJDUb7tavi5rIpoDQQadAKBvKGcvCNgCMlT5mMG03FD4NyoQyFfCZ9w76HiyMZJg6cwsS5-VtJg1Rs1xG80md1B8DrUGrSp8YeIBpxbrmK_8wpQPWjkMQdJQPpUX4FAOyq5Nt1Y1MbrEjd8j68CG15mtG8yWmnMrz3shNSf&uniplatform=NZKPT&language=CHS
|
[14] |
方长发, 马俪珍, 刘会平, 等. 固相微萃取技术及其在N-亚硝胺分析中的应用[J]. 肉类研究, 2008(4): 49-50. doi: 10.3969/j.issn.1001-8123.2008.04.014
FANG Changfa, MA Lizhen, LIU Huiping, et al. Solid phase microextraction (SPME) and its application in nitrosamine analysis[J]. Meat Res, 2008(4): 49-50. (in Chinese) doi: 10.3969/j.issn.1001-8123.2008.04.014
|
[15] |
陶燕飞, 黄红林, 张桃芝. 啤酒中N-亚硝胺的SPME-GC-MS分析[J]. 分析测试学报, 2003, 22(5): 82-84. doi: 10.3969/j.issn.1004-4957.2003.05.024
TAO Yanfei, HUANG Honglin, ZHANG Taozhi. Determination of volatile N-nitrosocompounds in beer by SPME-GC-MS[J]. J Instrumental Anal, 2003, 22(5): 82-84. (in Chinese) doi: 10.3969/j.issn.1004-4957.2003.05.024
|
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吴燕燕,曹松敏,李来好,杨贤庆,王锦旭,胡晓. 比较2种蓝圆鰺腌干工艺中脂质氧化与挥发性风味物质形成的关系. 食品科学. 2017(06): 165-172 .
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任中阳,吴燕燕,李来好,杨贤庆,戚勃,岑剑伟. 腌干鱼制品热泵干燥工艺参数优化. 南方水产科学. 2015(01): 81-88 .
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![]() | |
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![]() | |
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![]() | |
27. |
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![]() | |
28. |
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![]() | |
29. |
蔡秋杏,吴燕燕,李来好,杨贤庆,赵永强,王悦齐. 厦门白姑鱼腌制加工过程中的脂肪酸变化分析. 食品科学. 2015(12): 76-81 .
![]() | |
30. |
徐赛男,吴祖芳,陈杰. 气相色谱-质谱联用法测定传统腌菜中的N-亚硝胺. 食品与生物技术学报. 2015(11): 1162-1167 .
![]() | |
31. |
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![]() | |
32. |
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![]() | |
33. |
蔡秋杏,吴燕燕,李来好,杨贤庆,赵永强,王悦齐. 黄花鱼腌制加工过程的脂肪氧化分析. 食品安全质量检测学报. 2014(12): 4079-4084 .
![]() | |
34. |
黄超,迟原龙,黄紫霖,贾冬英,姚开. 植物乳杆菌AB-1降解亚硝酸钠的条件优化. 中国酿造. 2014(09): 13-16 .
![]() | |
35. |
吴燕燕,王雅楠,李来好,杨贤庆,戚勃,黄卉,马海霞. 咸鱼中戊糖片球菌产亚硝酸盐还原酶的条件优化. 食品工业科技. 2013(24): 195-199 .
![]() |